CN113185638A - High-toughness conductive nano composite ionic gel and preparation method thereof - Google Patents
High-toughness conductive nano composite ionic gel and preparation method thereof Download PDFInfo
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- CN113185638A CN113185638A CN202110449220.2A CN202110449220A CN113185638A CN 113185638 A CN113185638 A CN 113185638A CN 202110449220 A CN202110449220 A CN 202110449220A CN 113185638 A CN113185638 A CN 113185638A
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001879 gelation Methods 0.000 title description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002608 ionic liquid Substances 0.000 claims abstract description 31
- -1 acrylic ester Chemical class 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 21
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 18
- 239000003999 initiator Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010526 radical polymerization reaction Methods 0.000 claims description 13
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical group CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- CCJAYIGMMRQRAO-UHFFFAOYSA-N 2-[4-[(2-hydroxyphenyl)methylideneamino]butyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCCCN=CC1=CC=CC=C1O CCJAYIGMMRQRAO-UHFFFAOYSA-N 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical group OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- HFCUBKYHMMPGBY-UHFFFAOYSA-N 2-methoxyethyl prop-2-enoate Chemical compound COCCOC(=O)C=C HFCUBKYHMMPGBY-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 2
- 238000005273 aeration Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- VNXDRVGEKWGXAU-UHFFFAOYSA-N cyanocyanamide;1-ethyl-3-methyl-2h-imidazole Chemical compound N#CNC#N.CCN1CN(C)C=C1 VNXDRVGEKWGXAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000000499 gel Substances 0.000 description 69
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 16
- 238000003756 stirring Methods 0.000 description 13
- 238000009864 tensile test Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
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- 230000009471 action Effects 0.000 description 2
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- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- MKHFCTXNDRMIDR-UHFFFAOYSA-N cyanoiminomethylideneazanide;1-ethyl-3-methylimidazol-3-ium Chemical compound [N-]=C=NC#N.CCN1C=C[N+](C)=C1 MKHFCTXNDRMIDR-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 210000003813 thumb Anatomy 0.000 description 2
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 description 1
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- LRESCJAINPKJTO-UHFFFAOYSA-N bis(trifluoromethylsulfonyl)azanide;1-ethyl-3-methylimidazol-3-ium Chemical compound CCN1C=C[N+](C)=C1.FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F LRESCJAINPKJTO-UHFFFAOYSA-N 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006355 external stress Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 210000004247 hand Anatomy 0.000 description 1
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- 239000011159 matrix material Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229940088644 n,n-dimethylacrylamide Drugs 0.000 description 1
- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention provides a high-toughness conductive nano composite ionic gel and a preparation method thereof, wherein on the basis of ensuring the toughness of a product, the product has better conductivity and extensibility, excellent comprehensive performance and simple preparation process, and is suitable for large-scale production. A high-toughness conductive nano composite ionic gel is characterized in that: the preparation raw materials of the high-toughness conductive nano composite ionic gel comprise nano titanium dioxide hydrosol, ionic liquid and a monomer, wherein the volume ratio of the ionic liquid to the nano titanium dioxide hydrosol is 1-8: 1, mixing the components of the raw materials, wherein the molar concentration of a monomer is 0.5-3M; the particle size of the nano titanium dioxide in the nano titanium dioxide hydrosol is 5-30 nm, and the mass concentration of the nano titanium dioxide in the nano titanium dioxide hydrosol is 10-15%; the monomer is acrylic acid, acrylic ester or acrylamide monomer.
Description
Technical Field
The invention relates to the field of flexible electronic materials, in particular to a high-toughness conductive nano composite ionic gel and a preparation method thereof.
Background
In recent years, with the development of scientific technology and the improvement of living needs of people, various wearable flexible electronic devices are rapidly developed. However, the conventional conductive materials represented by metals have high modulus and poor extensibility, and cannot meet the requirements of flexible electronic equipment. Therefore, there is an urgent need to develop a flexible conductive material with excellent flexibility and ductility to meet the development requirements of the current wearable electronic devices.
The gel material is a soft material formed by a cross-linked polymer network and various liquids dispersed in the cross-linked polymer network, has excellent performances such as good flexibility and low modulus, can be prepared by using a conductive polymer or adding various conductive components into a liquid component, and is considered as an ideal material of flexible wearable electronic equipment. Among them, ionic gel using ionic liquid as conductive component has the advantages of high conductivity, good thermal stability and non-volatile liquid, and is one of the mainstream directions for conductive gel development at present. The prior art discloses methods for preparing Ionic gels, such as Zongxiao Li, Jinke Wang, Ruofei Hu, Chi Lv, and Junping Zheng, A Highly Ionic Conductive, Healable, and Adhesive polymeric-Supported Ionic gels, Macromolecular Rapid Communications,2019, 40, 1800776 (hereinafter referred to as document 1), Jianhang Liu1, Hongzan Song1, Ziha Wang1, Jianxin Zhang1, Jun Zhang2, Xinwu Ba1, Stretchable, self-Adhesive, and reproducible crystalline-linked Ionic gels, obtained from Jun Sanguin, Jun Xue Bu, Jun Xue Bu Xue Bu, Jun Xue Bu, Jun Xu Xue Bu Xue, Jun Xue Ying Xue No. 2, Jun Xue No. 2, Jun Xue No. Huang Xue No. 2, Jun Xue No. 2, Jun Xue Ying No. 2, though Xue, Jun Xue, though Xue, though Xue, though Xue, though Xue, though Xue, though Xue, though Xue, though, Xue, Xue, Xue, though Xue, though Xue, Xue, Xue, Xue, Xue, Xue, Xue, Xue, Xue, Xue, Xu, li Mei Zhang, Yuan He, Sibo Cheng, Hao Sheng, Keren Dai, Wen Jiang Zheng, Mei Xiaong Wang, Zhen Shann Chen, Yong Mei Chen, and Zhuangg Suo, Self-Healing, Adhesive, and high Strain noise as a strand Sensor for extreme Large Deformation, Small 2019, 15, 1804651 (hereinafter referred to as document 4). The conductivity and elongation of the ionic gel prepared in the above-mentioned document are shown below, respectively.
The ionic gels prepared by the methods related to the above documents 1 and 3 have low extensibility and conductivity, the ionic gels prepared by the methods related to the document 2 have low extensibility although the conductivity is greatly improved, and the ionic gels prepared by the methods related to the document 4 have low conductivity although the extensibility is greatly improved, so that the ionic gels cannot meet the requirements of practical application.
Disclosure of Invention
In order to overcome the defects of the prior art and better meet the development requirements of wearable electronic equipment, the invention provides the high-toughness conductive nano composite ionic gel and the preparation method thereof.
The technical scheme is that the high-toughness conductive nano composite ionic gel is characterized in that: the preparation raw materials of the high-toughness conductive nano composite ionic gel comprise nano titanium dioxide hydrosol, ionic liquid and a monomer, wherein the volume ratio of the ionic liquid to the nano titanium dioxide hydrosol is 1-8: 1, mixing the components of the raw materials, wherein the molar concentration of the monomer is 0.5-3M;
the particle size of the nano titanium dioxide in the nano titanium dioxide hydrosol is 5-30 nm, and the mass concentration of the nano titanium dioxide in the nano titanium dioxide hydrosol is 10-15%;
the monomer is one or the mixture of more than two of acrylic acid, acrylic ester or acrylamide monomers.
Further, the ionic liquid is one or a mixture of more than two of 1-methyl-3-butylimidazole tetrafluoroborate, 1-methyl-3-butylimidazole hexafluorophosphate, 1-ethyl-3-methylimidazole acetate, 1-methyl-butylimidazole hydrogen sulfate, 1-ethyl-3-methylimidazole bistrifluoromethylsulfonyl imide salt and 1-ethyl-3-methylimidazole dicyanamide salt;
the acrylate or acrylamide monomer is 2-hydroxyethyl acrylate, 2-methoxyethyl acrylate, acrylamide, N-isopropylacrylamide, N-dimethylacrylamide or N-methylolacrylamide.
Furthermore, the raw materials for preparing the high-toughness conductive nano-composite ionic gel also comprise an initiator and a catalyst,
the initiator is ammonium persulfate, potassium persulfate or sodium persulfate, and the amount of the initiator is 1-5% of the mass of the monomer;
the catalyst is N, N, N ', N' -tetramethyl ethylenediamine, and the dosage of the catalyst is 0.1-1% of the mass of the monomer.
A preparation method of high-toughness conductive nano composite ionic gel is characterized by comprising the following steps:
(1) mixing the nano titanium dioxide hydrosol with the ionic liquid to obtain uniform nano titanium dioxide ionic liquid dispersion liquid;
(2) adding the monomer into the nano titanium dioxide ionic liquid dispersion liquid, introducing inert gas to discharge oxygen in a system, adding an initiator and a catalyst, and carrying out free radical polymerization to obtain nano titanium dioxide crosslinked aqueous nano composite ionic gel, wherein the temperature of the free radical polymerization is 40-80 ℃, and the polymerization time is 4-12 hours;
(3) and (3) drying the nano titanium dioxide crosslinked hydrous nano composite ionic gel in vacuum, and removing water to obtain the high-toughness conductive nano composite ionic gel.
Preferably, in the step (1), the particle size of the nano titanium dioxide is 5-30 nm, and the nano titanium dioxide is rutile type.
Preferably, in the step (2), the inert gas is nitrogen or helium, and the aeration time of the inert gas is 20-60 minutes.
Preferably, in the step (2), the temperature of the free radical polymerization is 40-80 ℃, and the polymerization time is 4-12 hours.
Preferably, in the step (3), the vacuum drying temperature is 80 ℃ and the time is 2-8 hours.
Preferably, the average particle size of the nano titanium dioxide is 10 nm, and the mass concentration is 10%;
the ionic liquid is 1-methyl-3-butylimidazole hexafluorophosphate, and the volume is 35 ml;
the monomers are acrylamide and N-isopropyl acrylamide, the mole number of the acrylamide is 0.02 mol, and the mole number of the N-isopropyl acrylamide is 0.20 mol;
the initiator is ammonium persulfate with the mass of 0.1 g, and the catalyst is N, N, N ', N' -tetramethylethylenediamine with the mass of 25 mg.
Preferably, the average particle size of the nano titanium dioxide is 30 nm, and the mass concentration is 10%;
the ionic liquid is 1-methyl-butyl imidazole hydrogen sulfate, and the volume is 70 ml;
the monomers are acrylamide and N-hydroxymethyl acrylamide, the mole number of the acrylamide is 0.06 mol, and the mole number of the N-hydroxymethyl acrylamide is 0.1 mol;
the initiator is ammonium persulfate with the mass of 0.28 g, and the catalyst is N, N, N ', N' -tetramethylethylenediamine with the mass of 45 mg.
The high-toughness conductive nano composite ionic gel disclosed by the invention has the elongation at break of 526-2280%, the tensile strength of 153 kPa-1.13 MPa, and the conductivity of: 1.26 to 7.3S m-1. Compared with documents 1 and 3, the conductivity and the elongation of the high-toughness conductive nanocomposite ionic gel are greatly improved, compared with document 2, the elongation of the high-toughness conductive nanocomposite ionic gel is greatly improved, and compared with document 4, the conductivity of the high-toughness conductive nanocomposite ionic gel is greatly improved. Meanwhile, the high-toughness conductive nano composite ionic gel has better tensile strength, and the product has excellent comprehensive performance. In addition, the used raw materials are all commercialized products, and the preparation process is simple and suitable for large-scale production.
The high-toughness conductive nano composite ionic gel and the preparation method thereof have the following beneficial effects:
(1) the gel disclosed by the invention uses nano titanium dioxide as a multifunctional inorganic cross-linking agent, a multi-point non-covalent bond cross-linked structure is formed by the nano titanium dioxide and a polymerization product of acrylic acid, acrylic ester or acrylamide monomer, the nano titanium dioxide is uniformly dispersed in a polymer matrix, and the prepared ionic gel has a regular network structure, can uniformly bear external stress and prevents stress concentration; in addition, the reversible non-covalent crosslinking structure can be firstly broken when the ionic gel is subjected to external force, and energy is dissipated, so that the extensibility and the strength of the ionic gel are remarkably improved.
(2) The selected ionic liquid has moderate interaction with the polymer chain, so that the ionic liquid is not extruded out due to the action of external force in the using process, and meanwhile, the fluidity of anions and cations in a polymer network is ensured, and the ionic gel has excellent conductivity.
(3) Ionic gels of the inventionThe elongation at break is 526-2280%, the tensile strength is 153 kPa-1.13 MPa, and the conductivity is as follows: 1.26 to 7.3S m-1(ii) a Compared with documents 1 and 3, the ionic gel disclosed by the invention has greatly improved conductivity and elongation, compared with document 2, the ionic gel disclosed by the invention has greatly improved elongation, and compared with document 4, the ionic gel disclosed by the invention has greatly improved conductivity; meanwhile, the ionic gel has better tensile strength, and the product has excellent comprehensive performance.
(4) The ionic gel with high toughness and high conductivity is prepared by a simple free radical polymerization method, the preparation process is simple, and the used raw materials are the existing commercialized products and are suitable for large-scale production.
Drawings
FIG. 1 is a schematic view showing a state in which a spherical sample is manually pressed with a thumb according to example 1.
Fig. 2 is a schematic diagram of the state of the strip sample in example 1, wherein the sample is manually held and stretched at two ends, and the unstretched strip sample is arranged below the ruler.
FIG. 3 is a scanning electron micrograph of an ionic gel of example 1, with a scale unit of 10 μm.
FIG. 4 is a scanning electron micrograph of an ionic gel of example 1, with a scale unit of 5 μm.
Figure 5 is a tensile stress-strain curve for the ionic gel of example 1.
Detailed Description
1. Description of the raw materials
Nano TiO 22All purchased from Hangzhou Wanjing New Material Co Ltd, the specific models are as follows:
10 nm nanometer TiO2Model VK-TG01, powder.
15 nm nano TiO2Model VK-TA33, liquid, TiO2The mass concentration is 15%.
20 nm nanometer TiO2Model VK-TA31C, liquid, TiO2The mass concentration is 20%.
30 nm nanometer TiO2Model VK-TA31H, liquid, TiO2The mass concentration is 20%.
Nano TiO 22Sol preparation:
nano TiO with average grain size of 10 nm and mass concentration of 10%2Sol, 10 g VK-TG01 and 0.5g sodium pyrophosphate as dispersant were weighed out and added into a beaker filled with 90 ml deionized water, and ultrasonic dispersion was carried out at 25 ℃ for 2 hours to obtain 10% nano TiO required in example 12And (3) sol.
Nano TiO with average grain diameter of 15 nm and mass concentration of 10%2Dissolving sol, weighing 10 g VK-TA33, adding into a beaker, adding 5 ml deionized water, and performing ultrasonic dispersion at 25 ℃ for 2h to obtain 10% of nano TiO required in example 22And (3) sol.
Nano TiO with average grain diameter of 20 nm and mass concentration of 15%2Sol, weighing 75 g VK-TA31C, adding into a beaker, adding 25 ml deionized water, ultrasonic dispersing at 25 deg.C for 2h to obtain 15% nano TiO required in example 32And (3) sol.
Nano TiO with average grain diameter of 30 nm and mass concentration of 10%2Sol, weighing 50g VK-TA31H and 30 nm VK-TA31H, adding into a beaker, adding 50ml deionized water, and performing ultrasonic dispersion at 25 ℃ for 2h to obtain 10% of nano TiO required in example 42And (3) sol.
The ionic liquids used in the patents are all purchased from enokay chemical agents ltd, and the specific goods numbers are as follows:
1-methyl-3-butylimidazolium tetrafluoroborate, cat no: A43205.
1-methyl-3-butylimidazolium hexafluorophosphate, cat #: A33092.
1-ethyl-3-methylimidazole acetate, cat # s: A04875.
1-methyl-butylimidazolium bisulfate, cat no: A67440.
1-ethyl-3-methylimidazolium bistrifluoromethanesulfonimide salt, cat no: A79426.
1-ethyl-3-methylimidazolium dicyanamide salt, cat No.: A83377.
example 1
Taking 5 ml of the mixture with an average particle size of 10 nm and a mass concentration of 10%Nano TiO 22Adding the sol and 35 ml of ionic liquid 1-methyl-3-butylimidazolium hexafluorophosphate into a round-bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. 0.02 mol of acrylamide and 0.02 mol of N-isopropylacrylamide are added into the dispersion, the mixture is stirred for 40 minutes under the condition of introducing helium gas, 0.1 g of amine persulfate serving as an initiator and 25 mg of N, N, N ', N' -tetramethylethylenediamine serving as a catalyst are added, the mixture is stirred uniformly, then the mixture is transferred into molds with different shapes, sealed and subjected to free radical polymerization for 4 hours at the temperature of 80 ℃. And after the polymerization is finished, taking out the sample, and drying the sample in vacuum drying at 80 ℃ for 6 hours to constant weight to obtain a spherical sample and a strip sample of the high-toughness conductive nano composite ionic gel, wherein the diameter of the spherical sample is 2cm, the length of the strip sample is 10cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in the embodiment has uniform appearance and excellent mechanical properties, the spherical sample is manually pressed by a thumb, and the strip-shaped sample is manually stretched at two ends by hands, as shown in figures 1 and 2, the sample can bear large-scale stretching and compression without being broken, and the ionic liquid is not extruded due to the action of external force in the large-scale stretching and compression process.
The tensile test shows that (equipment test) the breaking elongation of the ionic gel is 1725%, the tensile strength is 475 kPa, and as shown in FIG. 5, the ionic liquid is not extruded due to the external force when the ionic liquid is detected by the detection equipment.
The observation of a scanning electron microscope shows that the ionic gel has a uniform three-dimensional network mechanism, as shown in fig. 3 and 4.
Conductivity tests showed that the conductivity of the ionic gel was 1.26S m-1Indicating that the mobility of the anions and cations in the polymer network is good.
The ionic gel prepared in this example had similar appearance and microstructure to the ionic gel prepared in example 1, and tensile testing showed that the ionic gel had an elongation at break of 2280%, a tensile strength of 153kPa, and a conductivity of 5.3S m-1。
Example 2
Taking 10 ml of the mixture with an average particle size of 15 nm nanometer TiO with mass concentration of 10%2Adding the sol and 40 ml of ionic liquid 1-methyl-3-butylimidazole tetrafluoroborate into a round bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. 0.01 mol of acrylic acid and 0.04 mol of N, N-dimethylacrylamide are added into the dispersion, the mixture is stirred for 30 minutes under the condition of introducing nitrogen, 0.15 g of initiator potassium persulfate and 20 mg of catalyst N, N, N ', N' -tetramethylethylenediamine are added, the mixture is stirred uniformly, then the mixture is transferred into molds with different shapes, sealed and subjected to free radical polymerization for 8 hours at the temperature of 60 ℃. And after the polymerization is finished, taking out the sample, and drying the sample in vacuum drying at 80 ℃ for 4 hours to constant weight to obtain a spherical sample and a strip sample of the high-toughness conductive nano composite ionic gel, wherein the diameter of the spherical sample is 2cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in this example has similar appearance and microstructure to the ionic gel prepared in example 1, and the tensile test shows that the ionic gel has an elongation at break of 1725%, a tensile strength of 475 KPa, and an electrical conductivity of 1.26S m-1。
Example 3
Taking 15 ml of nano TiO with the average grain diameter of 20 nm and the mass concentration of 15 percent2Adding the sol and 25 ml of ionic liquid 1-ethyl-3-methylimidazole acetate into a round-bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. Adding 0.04 mol of acrylic acid and 0.08 mol of 2-hydroxyethyl acrylate into the dispersion, stirring for 60 minutes under the condition of introducing nitrogen, adding 0.58 g of initiator sodium persulfate and 60 mg of catalyst N, N, N ', N' -tetramethylethylenediamine, stirring uniformly, transferring into molds of different shapes, sealing, and carrying out free radical polymerization for 12 hours at 40 ℃. And after the polymerization is finished, taking out the sample, and drying the sample in vacuum drying at 80 ℃ for 5 hours to constant weight to obtain a spherical sample and a strip sample of the high-toughness conductive nano composite ionic gel, wherein the diameter of the spherical sample is 2cm, the length of the strip sample is 10cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in this example had the same properties as the ionic gel prepared in example 1Similar appearance and microstructure, tensile testing showed the ionic gel to have an elongation at break of 526%, a tensile strength of 1.13MPa, and a conductivity of 4.5S m-1。
Example 4
10 ml of nano TiO with the average grain diameter of 30 nm and the mass concentration of 10 percent is taken2Adding the sol and 70ml of ionic liquid 1-methyl-butylimidazole hydrogen sulfate into a round-bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. Adding 0.06 mol of acrylamide and 0.1 mol of N-hydroxymethyl acrylamide into the dispersion, stirring for 20 minutes under the condition of introducing helium, adding 0.28 g of amine persulfate as an initiator and 45 mg of N, N, N ', N' -tetramethylethylenediamine as a catalyst, stirring uniformly, transferring into molds with different shapes, sealing, and carrying out free radical polymerization for 6 hours at 50 ℃. And after the polymerization is finished, taking out the sample, and drying the sample in vacuum drying at 80 ℃ for 5 hours to constant weight to obtain a spherical sample and a strip sample of the high-toughness conductive nano composite ionic gel, wherein the diameter of the spherical sample is 2cm, the length of the strip sample is 10cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in this example had similar appearance and microstructure to the ionic gel prepared in example 1, and tensile testing showed that the ionic gel had an elongation at break of 1150%, a tensile strength of 386 kPa, and a conductivity of 7.3S m-1。
Example 5
20 ml of nano TiO with the average grain diameter of 15 nm and the mass concentration of 15 percent is taken2Adding the sol and 40 ml of ionic liquid 1-ethyl-3-methylimidazolium bistrifluoromethylsulfonyl imide salt into a round-bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. 0.02 mol of acrylic acid and 0.1 mol of 2-methoxyethyl acrylate were added to the dispersion, and the mixture was stirred for 40 minutes under a nitrogen atmosphere, 0.23 g of ammonium persulfate as an initiator and 60 mg of N, N, N ', N' -tetramethylethylenediamine as a catalyst were added thereto, and after stirring the mixture uniformly, the mixture was transferred to molds of various shapes, sealed and subjected to radical polymerization at 70 ℃ for 4 hours. After the polymerization is finished, the sample is taken out and dried in vacuum drying at 80 ℃ for 8 hours until the temperature is constantAnd obtaining a spherical sample and a strip sample of the high-toughness conductive nanocomposite ionic gel, wherein the diameter of the spherical sample is 2cm, the length of the strip sample is 10cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in this example had similar appearance and microstructure to the ionic gel prepared in example 1, and tensile testing showed that the ionic gel had an elongation at break of 785%, a tensile strength of 560 kPa, and a conductivity of 1.8S m-1。
Example 6
5 ml of nano TiO with the average grain diameter of 15 nm and the mass concentration of 15 percent is taken2Adding the sol and 25 ml of ionic liquid 1-ethyl-3-methylimidazolium dicyanamide salt into a round-bottom flask, and magnetically stirring and mixing for 30 min to obtain uniform nano TiO2And (3) dispersing the mixture. Adding 0.03 mol of acrylic acid and 0.06 mol of acrylamide into the dispersion, stirring for 40 minutes under the condition of introducing helium, adding 0.13 g of amine persulfate serving as an initiator and 15 mg of N, N, N ', N' -tetramethylethylenediamine serving as a catalyst, stirring uniformly, transferring into molds with different shapes, sealing, and carrying out free radical polymerization for 7 hours at the temperature of 60 ℃. And after the polymerization is finished, taking out the sample, and drying the sample in vacuum drying at 80 ℃ for 4 hours to constant weight to obtain a spherical sample and a strip sample of the high-toughness conductive nano composite ionic gel, wherein the diameter of the spherical sample is 2cm, the length of the strip sample is 10cm, and the diameter of the strip sample is 6.3 mm.
The ionic gel prepared in this example had similar appearance and microstructure to the ionic gel prepared in example 1, and tensile testing showed that the ionic gel had an elongation at break of 1380%, a tensile strength of 496 kPa, and a conductivity of 3.2S m-1。
The invention is not limited to the examples given, and any equivalent alterations to the technical solution of the invention, which are made by those skilled in the art after reading the description of the invention, are covered by the claims of the invention.
Claims (10)
1. A high-toughness conductive nano composite ionic gel is characterized in that: the preparation raw materials of the high-toughness conductive nano composite ionic gel comprise nano titanium dioxide hydrosol, ionic liquid and a monomer, wherein the volume ratio of the ionic liquid to the nano titanium dioxide hydrosol is 1-8: 1, mixing the components of the raw materials, wherein the molar concentration of the monomer is 0.5-3M;
the particle size of the nano titanium dioxide in the nano titanium dioxide hydrosol is 5-30 nm, and the mass concentration of the nano titanium dioxide in the nano titanium dioxide hydrosol is 10-15%;
the monomer is one or the mixture of more than two of acrylic acid, acrylic ester or acrylamide monomers.
2. The high toughness conductive nanocomposite ionic gel of claim 1, wherein: the ionic liquid is one or the mixture of more than two of 1-methyl-3-butylimidazole tetrafluoroborate, 1-methyl-3-butylimidazole hexafluorophosphate, 1-ethyl-3-methylimidazole acetate, 1-methyl-butylimidazole hydrogen sulfate, 1-ethyl-3-methylimidazole bis (trifluoromethanesulfonyl) imide salt and 1-ethyl-3-methylimidazole dicyanamide salt;
the acrylate or acrylamide monomer is 2-hydroxyethyl acrylate, 2-methoxyethyl acrylate, acrylamide, N-isopropylacrylamide, N-dimethylacrylamide or N-methylolacrylamide.
3. A high toughness electrically conductive nanocomposite ionic gel according to claim 2, characterized in that: the raw materials for preparing the high-toughness conductive nano-composite ionic gel also comprise an initiator and a catalyst,
the initiator is ammonium persulfate, potassium persulfate or sodium persulfate, and the amount of the initiator is 1-5% of the mass of the monomer;
the catalyst is N, N, N ', N' -tetramethyl ethylenediamine, and the dosage of the catalyst is 0.1-1% of the mass of the monomer.
4. The preparation method of the high-toughness conductive nanocomposite ionic gel of claim 3, which is characterized by comprising the following steps:
(1) mixing the nano titanium dioxide hydrosol with the ionic liquid to obtain uniform nano titanium dioxide ionic liquid dispersion liquid;
(2) adding the monomer into the nano titanium dioxide ionic liquid dispersion liquid, introducing inert gas to discharge oxygen in a system, adding an initiator and a catalyst, and carrying out free radical polymerization to obtain nano titanium dioxide crosslinked aqueous nano composite ionic gel, wherein the temperature of the free radical polymerization is 40-80 ℃, and the polymerization time is 4-12 hours;
(3) and (3) drying the nano titanium dioxide crosslinked hydrous nano composite ionic gel in vacuum, and removing water to obtain the high-toughness conductive nano composite ionic gel.
5. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: in the step (1), the particle size of the nano titanium dioxide is 5-30 nm, and the nano titanium dioxide is rutile type.
6. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: in the step (2), the inert gas is nitrogen or helium, and the aeration time of the inert gas is 20-60 minutes.
7. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: in the step (2), the temperature of the free radical polymerization is 40-80 ℃, and the polymerization time is 4-12 hours.
8. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: in the step (3), the vacuum drying temperature is 80 ℃ and the time is 2-8 hours.
9. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: the average grain diameter of the nano titanium dioxide is 10 nm, and the mass concentration is 10%;
the ionic liquid is 1-methyl-3-butylimidazole hexafluorophosphate, and the volume is 35 ml;
the monomers are acrylamide and N-isopropyl acrylamide, the mole number of the acrylamide is 0.02 mol, and the mole number of the N-isopropyl acrylamide is 0.20 mol;
the initiator is ammonium persulfate with the mass of 0.1 g, and the catalyst is N, N, N ', N' -tetramethylethylenediamine with the mass of 25 mg.
10. The method for preparing the high-toughness conductive nanocomposite ionic gel according to claim 4, wherein the method comprises the following steps: the average grain diameter of the nano titanium dioxide is 30 nm, and the mass concentration is 10%;
the ionic liquid is 1-methyl-butyl imidazole hydrogen sulfate, and the volume is 70 ml;
the monomers are acrylamide and N-hydroxymethyl acrylamide, the mole number of the acrylamide is 0.06 mol, and the mole number of the N-hydroxymethyl acrylamide is 0.1 mol;
the initiator is ammonium persulfate with the mass of 0.28 g, and the catalyst is N, N, N ', N' -tetramethylethylenediamine with the mass of 45 mg.
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| CN114940729A (en) * | 2022-06-27 | 2022-08-26 | 燕山大学 | High-strength microphase separation ionic gel with anti-swelling characteristic and preparation method thereof |
| CN116023585A (en) * | 2022-12-30 | 2023-04-28 | 中国科学院兰州化学物理研究所 | Double-network NIPAM-based ionic gel and preparation method thereof |
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| CN102558412A (en) * | 2012-02-10 | 2012-07-11 | 北京理工大学 | Preparation method of high-strength titanium dioxide nano-grade composite hydrogel |
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